KR960010779A - 폴리이미드/실리카 복합체 및 그 필름의 제조방법 - Google Patents

폴리이미드/실리카 복합체 및 그 필름의 제조방법 Download PDF

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KR960010779A
KR960010779A KR1019950017504A KR19950017504A KR960010779A KR 960010779 A KR960010779 A KR 960010779A KR 1019950017504 A KR1019950017504 A KR 1019950017504A KR 19950017504 A KR19950017504 A KR 19950017504A KR 960010779 A KR960010779 A KR 960010779A
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paa
polyimide
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silica
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이용택
정화진
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이용택
김준웅
주식회사 선경인더스트리
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1057Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
    • C08G73/106Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain containing silicon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003Preparatory processes
    • C08G73/1007Preparatory processes from tetracarboxylic acids or derivatives and diamines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/54Silicon-containing compounds
    • C08K5/541Silicon-containing compounds containing oxygen
    • C08K5/5415Silicon-containing compounds containing oxygen containing at least one Si—O bond

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  • Chemical Kinetics & Catalysis (AREA)
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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

본 발명은 졸-겔(sol-gel)법에 의하여 폴리이미드(이하, PI라 함)/실리카 복합체내의 실리카 함량을 증가 시키고 상용성을 향상시키므로써 가교밀도가 높은 P I/실리카 복합체 및 그 필름의 제조방법에 관한 것으로, 다음과 같은 공정을 거쳐 제조된다.
1. 하기 구조식 (Ⅰ)로 나타내어지는 과량의 피로멜리트산이무수물(Pyromellitic dianhydride, PMDA)과 구조식 (Ⅱ)로 나타내어지는 옥시디아닐린(oxydianiline, ODA)를 N, N-디메틸아세트아미드(N,N-dimethylacetamide, DMAc) 용매하에서 반응시켜 적정수의 무수물 말단기를 갖는 폴리아믹산(polyamic acid, PAA)을 합성한 후,
2. 상기 공정에서 제조한 PAA에 실란 커플링제인 구조식 (Ⅲ)으로 나타내어지는 3-아미노프로필메틸디에 톡시실란(3-aminoprophylmethyl diethoxysilane, APMDS)을 첨가하여 PAA 사슬 말단을 봉쇄한 APMDS 봉지 PAA를 제조한 후,
3. 졸-겔 반응을 위하여 상기 ②공정의 APMDS 봉지 PAA 점성용액에 규정량의 구조식 (Ⅳ)로 나타내어지는 TEOS와 증류수를 첨가하고 균일하게 교반하여 실라놀 그룹을 형성시켜, P I/실리카 복합체의 점성용액을 제조하고,
4. 통상의 용액 캐스팅 방법에 의해 유리판에 캐스팅한 후 60℃에서 건조시키고 270℃에서 열처리하여 이미드화 및 중축합 반응을 시켜 P I/실리카 필름을 제조한다.

Description

폴리이미드/실리카 복합체 및 그 필름의 제조방법
본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음

Claims (5)

  1. 가)하기 구조식(Ⅰ)로 나타내어지는 피로멜리트산 이무수물(Pyromellitic dianhydride, PMDA) 과량과 구조식(Ⅱ)로 나타내어지는 옥시디아닐린(Oxydianiline, ODA)을 N,N-디메틸아세트아미드(N,N-dimethylacetamide, DMAc) 용매하에서 반응시켜 적정수의 무수물 말단기를 갖는 폴리아믹산(polyamic acid, PAA)을 합성한 후, 나) 상기 가)공정에서 제조한 PAA에 실란 커플링제인 구조식(Ⅲ)으로 나타내어지는 3-아미노프로필메틸디에톡시실란(3-aminopropylmethyldiethoxysilane, APMDS)을 말단기 작용기의 몰수와 같은 몰수 첨가하여 PAA를 제조한 후, 다) 졸-겔 반응을 위하여 상기 나)공정의 APMDS 봉지 PAA 점성용액에 규정량의 구조식(Ⅳ)로 나타내어지는 TEOS와 증류수를 첨가하고 균일하게 교반하여 실라놀 그룹을 형성시켜 제조함을 특징으로 하는 폴리이미드/실리카 복합체.
  2. 제1항에 있어서, ODA에 대한 PDMA의 반응 양론비는 1몰% 과량이며, 반응시간은 2~3시간이 최적반응 시간임을 특징으로 하는 폴리이미드/실리카 복합체.
  3. 제1항에 있어서, 폴리이미드/실리카 복합체내의 실리카 함량이 30~40중량% 되도록 TEOS를 첨가함을 특징으로 하는 폴리이미드/실리카 복합체.
  4. 제1항의 폴리이미드/실리카 복합체 점성용액을 통상적인 용액 캐스팅 방식에 의하여 캐스팅한 후 건조시키고 열처리하여 이미드화 및 증축반응시켜 제조함을 특징으로 하는 폴리이미드/실리카 복합필름의 제조방법.
  5. 제4항에 있어서, 열처리는 270℃이상에서 행함을 특징으로 하는 폴리이미드/실리카 복합필름의 제조방법.
    ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.
KR1019950017504A 1994-09-14 1995-06-26 폴리이미드/실리카 복합체 및 그 필름의 제조방법 Ceased KR960010779A (ko)

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KR94-23271 1994-09-14
KR19940023271 1994-09-14

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8399593B2 (en) 2009-10-30 2013-03-19 Samsung Electronics Co., Ltd. Polymer, and composition and film including the same
KR101430974B1 (ko) * 2007-12-27 2014-08-19 에스케이씨코오롱피아이 주식회사 폴리이미드 필름 및 그 제조방법

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6114156A (en) * 1996-10-31 2000-09-05 The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration Molecular level coating for metal oxide particles
TWI298076B (en) * 2004-04-30 2008-06-21 Eternal Chemical Co Ltd Precursor solution for polyimide/silica composite material, its manufacture method and polyimide/silica composite material having low volume shrinkage
JP2007246772A (ja) * 2006-03-17 2007-09-27 Nagoya Industrial Science Research Inst 多分岐ポリイミド系ハイブリッド材料
JP5883566B2 (ja) * 2011-02-18 2016-03-15 イビデン株式会社 多分岐ポリイミド系ハイブリッド材料の製造方法
WO2014003451A1 (en) * 2012-06-29 2014-01-03 Kolon Industries, Inc. Polyimide and polyimide film comprising the same
EP2690124B1 (en) * 2012-07-27 2015-09-16 Samsung Electronics Co., Ltd Composition Comprising Polyimide Block Copolymer And Inorganic Particles, Method Of Preparing The Same, Article Including The Same, And Display Device Including The Article
CN103483585B (zh) * 2013-09-13 2016-01-20 华南师范大学 高强高模有机硅改性PI/SiO2杂化薄膜的制备方法
KR102225510B1 (ko) * 2014-06-16 2021-03-08 삼성전자주식회사 폴리이미드-무기물 복합재료 제조용 조성물, 및 상기 조성물로부터 제조되는 성형품
CN108793895A (zh) * 2018-08-25 2018-11-13 北京建工新型建材有限责任公司 一种高抗裂性混凝土
JP7823796B2 (ja) * 2023-11-29 2026-03-04 日産化学株式会社 有機酸を含む窒素含有有機溶媒に分散したシリカゾル及び絶縁性樹脂組成物

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101430974B1 (ko) * 2007-12-27 2014-08-19 에스케이씨코오롱피아이 주식회사 폴리이미드 필름 및 그 제조방법
US8399593B2 (en) 2009-10-30 2013-03-19 Samsung Electronics Co., Ltd. Polymer, and composition and film including the same

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